CN114634180B - Super-microporous activated carbon material, preparation method thereof and application thereof in separation of light hydrocarbon compounds - Google Patents
Super-microporous activated carbon material, preparation method thereof and application thereof in separation of light hydrocarbon compounds Download PDFInfo
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a super-microporous activated carbon material, a preparation method thereof and application thereof in separation of light hydrocarbon compounds, and belongs to the technical field of separation of light hydrocarbon compounds of activated carbon materials. The invention selects chitosan as a carbon source, and the chitosan as the carbon source is a natural biological polymer, has wide sources and contains rich hydroxyl and amino functional groups, and provides favorable conditions for carbonization of the chitosan applied to adsorption separation of light hydrocarbons; KOH is selected as a pore-forming agent, chitosan is subjected to pre-carbonization treatment, then the pore-forming agent is added, and then complete carbonization treatment is carried out, so that a series of ultra-microporous carbon materials with high-quality light hydrocarbon compound separation performance are creatively synthesized. The method is simple to operate, has low requirements on equipment, and is suitable for industrial mass production.
Description
Technical Field
The invention belongs to the technical field of separation of light hydrocarbon compounds of activated carbon materials, and particularly relates to a super-microporous activated carbon material, a preparation method thereof and application thereof in separation of light hydrocarbon compounds.
Background
Light hydrocarbon is used as an important chemical raw material and widely applied to the fields of petrochemical industry, organic synthesis, medical synthesis, agriculture and the like, wherein the separation of olefin/alkane is called one of seven most important chemical separation processes. Typically, they are obtained by steam cracking or thermal decomposition of industrial heavy oils, accounting for 10% -15% of the global energy consumption, with global annual yields of ethylene exceeding 1.7 million tons, for example, for industrial separation of ethylene and ethane, due to ethane
And ethylene->
Is similar in molecular dynamics diameter, and pyrolysis of ethane produces ethylene, typically a mixture of ethane and ethylene. Existing commercial separations of ethane and ethylene require low temperature distillation at high pressure and low temperature for polymer grade ethylene production. Therefore, the traditional industrial separation process is huge in energy consumption, and the cost of the rectifying tower is quite high. For such energy-intensive and capital-intensive industrial processes, developing energy-efficient separation/purification techniques would greatly reduce global energy consumption and environmental pollution.
The adoption of non-thermal separation technologies such as membrane separation and adsorption is more energy-saving and the occupied area of equipment is smaller than that of traditional high-temperature low-pressure separation. The active carbon material is used as an ancient and effective adsorption material, is widely applied to the field of gas separation, has the advantages of low cost, good stability, easy regeneration and the like, and can realize effective adsorption and separation of target gas by preparing active carbon materials with different apertures and functional groups. However, for some light hydrocarbons with very similar physical and chemical properties, such as ethylene and ethane, the traditional carbon materials have difficulty in realizing effective separation of the two due to the very similar physical and chemical properties such as molecular size, boiling point and the like, and equilibrium adsorption parameters and the like. Therefore, the development and preparation of novel microporous activated carbon materials for adsorption separation of low-carbon hydrocarbons are extremely critical.
At present, few ultramicropore carbon materials are used for adsorption separation of light hydrocarbons, and most reported carbon materials lack specific properties for C because of irregular pore size distribution (0.5-100 nm) 2 H 6 The pore environment of specific adsorption, which results in its targeting C 2 H 6 /C 2 H 4 Is poor in selectivity of C 2 H 6 The adsorption capacity is low.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a super-microporous activated carbon material (C-CTS series), a preparation method thereof and application thereof in light hydrocarbon compound separation, which can effectively solve the problem that the traditional carbon material has poor selectivity on light hydrocarbon compound separation.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
the invention discloses a preparation method of a super-microporous activated carbon material, which comprises the following steps:
1) Performing preliminary carbonization treatment on chitosan to serve as a carbon source substrate;
2) Fully and uniformly mixing a carbon source substrate and a pore-forming agent, performing complete carbonization treatment, washing the product to be neutral by using pickling solution, and then drying to obtain the ultra-microporous active carbon material.
Preferably, in step 1), the pore-forming agent used is KOH, naOH, K 2 CO 3 And the like.
Preferably, in step 1), the preliminary carbonization treatment is to treat chitosan under nitrogen or inert atmosphere for 1 hour at a temperature rising rate of 1 ℃/min from room temperature to 500 ℃.
Further preferably, the inert atmosphere is argon, helium or the like.
Preferably, in the step 2), the mass ratio of the pore-forming agent to the carbon source substrate is (1-6): 1.
further preferably, the mass ratio of pore former to carbon source substrate is 1:1, 2:1, 4:1 or 6:1.
Preferably, in the step 2), the operation modes of fully and uniformly mixing are two modes: the carbon source substrate and the pore-forming agent are sufficiently ground for 30 to 60 minutes, or the substrate and the pore-forming agent are subjected to hydrothermal reaction for 24 hours at 85 ℃.
Preferably, in the step 2), the complete carbonization treatment is to treat the uniformly mixed sample at 500-800 ℃ for 1-3 hours.
Preferably, in the step 2), the washing is performed by heating and stirring with a large amount of deionized water, adding an acid washing solution, and filtering at a temperature of 85 ℃ for 12 hours.
Further preferably, the pickling solution is hydrochloric acid, nitric acid or sulfuric acid, and the concentration of the pickling solution is 1mol/L.
Preferably, in step 2), the drying is carried out in a vacuum oven for 24-72 hours.
The invention also disclosesThe specific surface area of the super-microporous activated carbon material prepared by the preparation method is 1883-3483m 2 And/g, pore diameter of 0.4-0.5nm, and the surface of the pore has rich N, O hetero atoms.
The invention also discloses application of the super-microporous activated carbon material in preparing an adsorbent for selectively adsorbing and separating light hydrocarbon compounds.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the super-microporous active carbon material, chitosan is selected as a carbon source, and the chitosan serving as the carbon source is a natural biological polymer, is wide in source, contains rich hydroxyl and amino functional groups, and provides favorable conditions for carbonization of the super-microporous active carbon material applied to adsorption separation of light hydrocarbons; the chitosan is subjected to pre-carbonization treatment, then the pore-forming agent is added, and then complete carbonization treatment is carried out, so that a series of ultra-microporous carbon materials with high-quality light hydrocarbon compound separation performance are creatively synthesized. The method is simple to operate, has low requirements on equipment, and is suitable for industrial mass production.
Further, by adjusting the addition amount of the pore-forming agent and the carbonization temperature, a microporous carbon material which can generate different interactions with different guest molecules can be constructed, thereby improving the selective adsorption capacity for specific gases.
The chitosan-based ultra-microporous activated carbon material prepared by the method has the advantages of ultra-high specific surface area, proper pore diameter and proper pore chemical environment (the pore surface is rich in N, O and other hetero atoms), and can be modified according to specific functional groups to prepare the ultra-microporous carbon material with different gas adsorption selectivities, so that the applicability of the C-CTS ultra-microporous carbon material is further improved. It is notable that the novel ultra-microporous carbon material has ultra-high specific surface area and proper pore size distribution, and the hydroxyl and amino functional groups which are not completely carbonized are also beneficial to the selective adsorption separation of light hydrocarbons.
The ultra-microporous activated carbon material prepared by the invention has the advantages of high performance on various light hydrocarbon compounds (C1 hydrocarbon/C2 hydrocarbon/C3 hydrocarbon/C4 hydrocarbon/CO 2 Acetylene, etc.) has good separation properties. The prepared ultra-microporous carbon material has unique reverse adsorption effect and strong adsorption capacity on specific gas molecules through pore size screening and the influence of N, O and other heteroatoms at room temperature, so that the ultra-microporous carbon material has excellent mixed gas separation performance. The synthesized novel ultra-microporous carbon material can effectively solve the problems of high energy consumption, poor separation effect, high equipment cost and the like of the traditional industrial light hydrocarbon separation, and greatly improves the application prospect of the carbon material in the light hydrocarbon separation field.
Drawings
FIG. 1 is an SEM image of C-CTS-2 prepared in example 1;
FIG. 2 is a powder X-ray diffraction pattern of C-CTS-2 prepared in example 1;
FIG. 3 is 77K N of C-CTS-2 prepared in example 1 2 An adsorption graph;
FIG. 4 is a graph of C-CTS-2 prepared in example 1 at 273 and 298K for C 2 H 6 Adsorption curve of (2);
FIG. 5 is a graph of C-CTS-2 prepared in example 1 at 273 and 298K for C 2 H 4 Adsorption curve of (2).
Detailed Description
In order that those skilled in the art will better understand the present invention, a technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in which it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and the claims of the present invention and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate such that the embodiments of the invention described herein may be implemented in sequences other than those illustrated or otherwise described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the attached drawing figures:
example 1
The preparation method of the ultra-microporous carbon material and the application of the separation of the light hydrocarbon compound are as follows: 2g of chitosan was placed in a tube furnace and pre-carbonized at 500℃for 1 hour in an argon (Ar) atmosphere, wherein the argon flow rate was 200mL min –1 The method comprises the steps of carrying out a first treatment on the surface of the Uniformly mixing the pre-carbonized chitosan carbon material and a pore-forming agent KOH according to the mass ratio of 1:2, placing the mixture in a mortar, grinding for 30-60 minutes to obtain compact powder (the powder state is observed in grinding, grinding can be stopped when no macroscopic particles exist), then placing the compact powder in a tubular furnace, and carbonizing the compact powder in an argon (Ar) atmosphere at 600 ℃ for 1 hour, wherein the argon flow rate is 300mL min –1 Grinding the obtained carbide for about 30-60 minutes after cooling to room temperature (the time is in an interval range because the powder state needs to be observed during grinding and grinding can be stopped when no macroscopic particles exist), then adding a large amount of deionized water for heating and stirring at the temperature of 85 ℃ for 12 hours, and preparing a 1M HCl solution for washing until the pH value is adjusted to 7; after filtration and washing, the obtained carbon material was dried in a vacuum oven at 100℃for 24 hours, and then left at room temperature for 2 hours, to obtain activated C-CTS-2 for the next gas adsorption separation experiment.
FIG. 1 is an SEM image of C-CTS-2 prepared in example 1;
FIG. 2 is a powder X-ray diffraction pattern of C-CTS-2 prepared in example 1, showing that all samples were at 2θ≡23.8 ° And 45 (V) ° Two similar broad peaks appear, corresponding to diffraction peaks of amorphous graphitic carbon; 23.8 ° Broad peak correspondence at (00)2) Diffraction plane, 45 ° The broad peak at the position corresponds to a (100) diffraction surface, and no diffraction peak except for a carbon peak shows that the hydrothermal acid washing completely removes K + And Cl - Ions.
FIG. 3 is 77K N of C-CTS-2 prepared in example 1 2 Adsorption isotherm patterns, BET up to 2906m, can be seen 2 /g。
FIG. 4 is a C-CTS-2 vs. C prepared in example 1 2 H 6 Is shown for C at 298K 2 H 6 Can reach a maximum adsorption capacity of 165.51cm 3 /g。
FIG. 5 is a C-CTS-2 vs. C prepared in example 1 2 H 4 The adsorption curve of (C) shows that the maximum adsorption amount is 124.92cm 3 /g, lower than that of C 2 H 6 Can realize reverse adsorption.
Example 2
The preparation method of the ultra-microporous carbon material and the application of the separation of the light hydrocarbon compound are as follows: 2g of chitosan was placed in a tube furnace and pre-carbonized at 500℃for 1 hour in an argon (Ar) atmosphere, wherein the argon flow rate was 200mL min –1 The method comprises the steps of carrying out a first treatment on the surface of the Uniformly mixing the pre-carbonized chitosan carbon material and a pore-forming agent KOH according to the mass ratio of 1:1, placing the mixture in a mortar, grinding for 30-60 minutes to obtain compact powder (the powder state is observed during grinding, grinding can be stopped when no macroscopic particles exist), then placing the compact powder in a tubular furnace, and carbonizing for 1 hour at 500 ℃ in an argon (Ar) atmosphere, wherein the argon flow rate is 300mL min –1 Grinding the obtained carbide for about 40-60 minutes after cooling to room temperature, adding a large amount of deionized water, heating and stirring at 85 ℃ for 12 hours, and washing the carbide until the pH value is regulated to 7 by preparing 1M HCl solution; the carbon material obtained after filtration and washing is dried in a vacuum oven at 100 ℃ for 24 hours and then is placed at room temperature for 2 hours, so that activated C-CTS-1 can be obtained for the next gas adsorption and separation experiment.
Example 3
The preparation method of the ultra-microporous carbon material and the application of the separation of the light hydrocarbon compound are as follows: 2g of chitosan was placed onPre-carbonizing in a tubular furnace at 500 deg.C under argon (Ar) atmosphere for 1 hr, wherein the argon flow rate is 200mL min –1 The method comprises the steps of carrying out a first treatment on the surface of the Uniformly mixing a pre-carbonized chitosan carbon material and a pore-forming agent NaOH according to a mass ratio of 1:4, placing the mixture in a mortar, grinding for 30-60 minutes to obtain compact powder (the powder state is observed during grinding, grinding can be stopped when no macroscopic particles exist), placing the compact powder in a tubular furnace, and carbonizing the compact powder in an argon (Ar) atmosphere at 700 ℃ for 1 hour, wherein the argon flow rate is 300mL min –1 Grinding the obtained carbide for about 40-60 minutes after cooling to room temperature, adding a large amount of deionized water, heating and stirring at 85 ℃ for 12 hours, and washing the carbide until the pH value is regulated to 7 by preparing 1M HCl solution; the carbon material obtained after filtration and washing is dried in a vacuum oven at 100 ℃ for 24 hours and then is placed at room temperature for 2 hours, so that activated C-CTS-4 can be obtained for the next gas adsorption and separation experiment.
Example 4
The preparation method of the ultra-microporous carbon material and the application of the separation of the light hydrocarbon compound are as follows: 2g of chitosan was placed in a tube furnace and pre-carbonized at 500℃for 1 hour in an argon (Ar) atmosphere, wherein the argon flow rate was 200mL min –1 The method comprises the steps of carrying out a first treatment on the surface of the Uniformly mixing the pre-carbonized chitosan carbon material and a pore-forming agent KOH according to the mass ratio of 1:6, placing the mixture in a mortar, grinding for 30-60 minutes to obtain compact powder (the powder state is observed during grinding, grinding can be stopped when no macroscopic particles exist), then placing the compact powder in a tubular furnace, and carbonizing the compact powder in an argon (Ar) atmosphere at 600 ℃ for 1 hour, wherein the argon flow rate is 300mL min –1 Grinding the obtained carbide for about 40-60 minutes after cooling to room temperature, adding a large amount of deionized water, heating and stirring at 85 ℃ for 12 hours, and washing the carbide until the pH value is regulated to 7 by preparing 1M HCl solution; the carbon material obtained after filtration and washing is dried in a vacuum oven at 100 ℃ for 24 hours and then is placed at room temperature for 2 hours, so that activated C-CTS-6 can be obtained for the next gas adsorption and separation experiment.
Example 5
Preparation method of ultra-microporous carbon material and separation of light hydrocarbon compoundThe application is specifically as follows: 2g of chitosan was placed in a tube furnace and pre-carbonized at 500℃for 1 hour in an argon (Ar) atmosphere, wherein the argon flow rate was 200mL min –1 The method comprises the steps of carrying out a first treatment on the surface of the Pre-carbonizing chitosan carbon material and pore-forming agent K 2 CO 3 Uniformly mixing according to the mass ratio of 1:2, placing the mixture into a 100mL hydrothermal reaction kettle, and reacting for 24 hours at 85 ℃; after cooling to room temperature, placing the mixture in a vacuum oven, and drying at 110 ℃ to obtain powder; the obtained powder was placed in a tube furnace and carbonized at 600℃for 1 hour in an argon (Ar) atmosphere at a flow rate of 300mL min –1 Grinding the obtained carbide for about 30-60 minutes after cooling to room temperature (powder state is observed during grinding, grinding can be stopped when no particles are visible to naked eyes), then adding a large amount of deionized water for heating and stirring, wherein the temperature is 85 ℃ and the time is 12 hours, and 1M HCl solution is prepared for washing until the pH value is adjusted to 7; the carbon material obtained after filtration and washing is dried in a vacuum oven at 100 ℃ for 24 hours and then is placed at room temperature for 2 hours, so that activated C-CTS-2 (hydrothermal method) can be obtained for the next step of functional group modification and other experiments.
In summary, the invention aims at the problem of poor separation selectivity of the traditional carbon material on the light hydrocarbon compound, selects chitosan as a carbon source, and creatively synthesizes a series of novel super-microporous active carbon materials with different specific surface areas, pore size distribution and N, O content by adjusting pore formers (such as KOH) and carbonization temperature. The novel activated carbon materials have good chemical stability and huge specific surface area, and can be further modified in a functional way according to the application, so that the super-microporous activated carbon materials with different specific surface areas and surface functional groups are synthesized, and the selective adsorption separation and purification of different types of low-carbon hydrocarbon compounds are realized. The method can be used for synthesizing a series of ultra-microporous activated carbon materials with high-efficiency light hydrocarbon compound separation effect, and has wide application potential and value.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (7)
1. The preparation method of the ultra-microporous activated carbon material is characterized by comprising the following steps of:
1) Performing preliminary carbonization treatment on chitosan to serve as a carbon source substrate;
the primary carbonization treatment is to heat chitosan to 500 ℃ from room temperature under nitrogen or inert atmosphere at a heating rate of 1 ℃/min for 1 hour;
2) Fully and uniformly mixing a carbon source substrate and a pore-forming agent, performing complete carbonization treatment, washing a product to be neutral by using pickling solution, and then drying to obtain a super-microporous active carbon material;
the mass ratio of the pore-forming agent to the carbon source substrate is (1-6): 1, a step of; the complete carbonization treatment is to treat the uniformly mixed sample at 500-800 ℃ for 1-3 hours.
2. The method for preparing a class of ultra-microporous activated carbon materials according to claim 1, wherein in step 2), the mass ratio of pore-forming agent to carbon source substrate is 1:1, 2:1, 4:1 or 6:1.
3. The method for preparing a class of ultra-microporous activated carbon materials according to claim 1, wherein in step 2), the operation modes of fully and uniformly mixing are two: the carbon source substrate and the pore-forming agent are sufficiently ground for 30 to 60 minutes, or the substrate and the pore-forming agent are subjected to hydrothermal reaction for 24 hours at 85 ℃.
4. The method for preparing a class of ultra-microporous activated carbon materials according to claim 1, wherein in step 2), the washing is performed by heating and stirring with a large amount of deionized water, adding pickling solution, at a temperature of 85 ℃ for 12 hours, and then suction-filtering; the pickling solution is hydrochloric acid, nitric acid or sulfuric acid, and the concentration of the pickling solution is 1mol/L.
5. The method for preparing a class of ultra microporous activated carbon materials according to claim 1, wherein in step 2), the drying is performed in a vacuum oven for 24-72 hours.
6. A class of ultra-microporous activated carbon materials prepared by the preparation method according to any one of claims 1 to 5, characterized in that the specific surface area of the ultra-microporous activated carbon material is 1883 to 3483m 2 Per g, the pore surface with the pore diameter of 0.4-0.5nm has rich N, O hetero atoms.
7. The use of a class of ultra microporous activated carbon materials according to claim 6 in the preparation of adsorbents for the selective adsorption separation of light hydrocarbon compounds.
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